Tantalate near-infrared fluorescent material and preparation method thereof

Abstract

The present invention discloses a tantalate near-infrared fluorescent material and a preparation method thereof, belonging to the field of near-infrared photoluminescence fluorescence technology. The present invention adopts a solid phase method to prepare the tantalate near-infrared fluorescent material, and its chemical formula is Ga 1‑x TaO4:xNi 2+ , wherein 0<x≤0.01. The present invention obtains Ga by Ni doping GaTaO4 1‑ x TaO4:xNi 2+ It can emit near-infrared light of 1541nm-1566nm, with high luminous efficiency and long luminous life. It can match commercial purple light chips to emit purple light with an emission center near 428nm, and emit near-infrared light of about 1541nm-1566nm. It has broad application prospects in the fields of lighting and display lighting.

Description

Technical Field

[0001] The invention belongs to the technical field of near-infrared photoluminescence fluorescence, and in particular relates to a tantalate near-infrared fluorescent material and a preparation method thereof. Background Art

[0002] As a new generation of luminescent materials, metal oxides have significant advantages in the following aspects: ① Efficient luminescence: Metal oxides can emit light by exciting electronic transitions, and their internal energy level structure and electronic band structure enable them to produce efficient luminescence effects. This makes metal oxides a very bright and efficient luminescent material. ② High stability: Metal oxides generally have high stability in high temperature and humid environments. Compared with other luminescent materials, the luminescence properties of metal oxides are not easily attenuated under long-term use and harsh environments. This gives metal oxides a longer service life in various applications. ③ Wide luminescence spectrum range: Metal oxides can achieve wide-band luminescence by adjusting their chemical composition and crystal structure. This allows metal oxides to emit multiple wavelengths of light, from ultraviolet to visible light and infrared. This property makes metal oxides have a wide range of application potential in different fields. ④ Adjustability: The luminescence properties of metal oxides can be customized by adjusting their composition, crystal structure and impurity doping. This means that metal oxide materials can be designed and synthesized according to specific needs to achieve the desired luminescence properties, such as luminescence intensity, wavelength and luminescence time. ⑤ Rich application fields: Metal oxides have a wide range of application potential. They can be used in lighting and display technologies such as light-emitting diodes (LEDs) and organic light-emitting diodes (OLEDs), as well as in bioimaging, sensors, photovoltaic devices, etc. The luminescent properties of metal oxides make them important for application in many different fields.

[0003] Therefore, as a new generation of luminescent materials, metal oxides have the advantages of high efficiency luminescence, high stability, wide luminescence spectrum range, controllability and a wide range of applications, making metal oxides an ideal choice for various optoelectronic and optical applications.

[0004] However, existing tantalate structured materials still have some shortcomings, including low luminous efficiency, high cost, short luminous lifetime, emission peak wavelength mostly concentrated within 800nm, and narrow near-infrared emission half-width. Summary of the invention

[0005] In view of the above-mentioned shortcomings of the prior art, the present invention provides a tantalate near-infrared fluorescent material and a preparation method thereof.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] A tantalate near-infrared fluorescent material, whose chemical formula is Ga1-x TaO4:xNi 2+ , where 0<x≤0.01.

[0008] As a preferred embodiment of the present invention, the tantalate near-infrared fluorescent material generates near-infrared light with a luminescent center of an emission peak located at 1541nm-1566nm under excitation of light with a wavelength of 428nm.

[0009] More preferably, the tantalate near-infrared fluorescent material generates near-infrared light with an emission peak centered at 1566 nm when excited by light with a wavelength of 428 nm.

[0010] A method for preparing a tantalate near-infrared fluorescent material comprises the following steps:

[0011] (1) Mix Ga2O3, Ta2O5 and NiO raw materials, add anhydrous ethanol and grind;

[0012] (2) Then calcining and cooling to obtain tantalate near-infrared fluorescent material.

[0013] As a preferred embodiment of the present invention, the heating rate of the calcination is 5°C / min, the calcination temperature is 1300-1500°C, and the calcination time is 1-5h.

[0014] As a preferred embodiment of the present invention, the volume ratio of the total mass of the raw material mixture to anhydrous ethanol is 1g: (4-7)ml.

[0015] As a preferred embodiment of the present invention, the grinding time is 20-60 minutes.

[0016] As a preferred embodiment of the present invention, the calcination atmosphere is at least one of air, nitrogen and argon.

[0017] As a preferred embodiment of the present invention, the purity of the Ga2O3, Ta2O5 and NiO raw materials is 99.99%.

[0018] Compared with the prior art, the invention has the following beneficial effects: the invention obtains GaTaO4 by Ni doping 1-x TaO4:xNi 2+ , where Ni replaces gallium, causing lattice expansion, and the change in material structure causes the luminescence peak to redshift, so that the material emits near-infrared light of 1541nm-1566nm at an excitation wavelength of 428nm, with high luminescence intensity and long luminescence lifetime. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is the XRD pattern of the tantalate near-infrared fluorescent material prepared in Example 1.

[0020] Figure 2 This is a photoluminescence image of the tantalate near-infrared fluorescent material prepared in Example 1 under the excitation of a xenon lamp with a wavelength of 428 nm as a light source at room temperature.

[0021] Figure 3 This is the excitation spectrum of the tantalate near-infrared fluorescent material prepared in Example 1.

[0022] Figure 4 This is a comparison chart of the relative luminescence intensity of the tantalate near-infrared fluorescent materials prepared in Examples 1-3. DETAILED DESCRIPTION

[0023] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0024] Example 1

[0025] A method for preparing a tantalate near-infrared fluorescent material, comprising the following preparation method:

[0026] (1) After mixing 24.9 mmol Ga2O3, 25 mmol Ta2O5, and 0.2 mmol NiO, the mixed powder was placed in an agate mortar, and an appropriate amount of anhydrous ethanol was dropped into it and then ground for 30 minutes; the volume ratio of the total mass of the mixed raw materials to the anhydrous ethanol was 1 g:4 ml.

[0027] (2) The ground powder is placed in a 70°C drying oven for half an hour, taken out and ground again until the material is in powder form, then the material is transferred to a corundum crucible, placed in a tubular furnace and heated at a rate of 5°C / min, sintered at 1500°C for 4 hours, and finally naturally cooled to room temperature to obtain a tantalate near-infrared fluorescent material.

[0028] according to Figure 1 It can be seen that Example 1 successfully prepared the tantalate near-infrared fluorescent material Ga with good crystallinity. 1-x TaO4:xNi 2 + .

[0029] according to Figure 2 It can be seen that under 428nm light excitation, the photoluminescence spectrum of the prepared tantalate near-infrared fluorescent material is a broadband near-infrared light with an emission center at 1542nm, and its half-peak width reaches a broadband near-infrared light of 1542nm. The relative luminescence intensity is shown in Figure 4 .

[0030] according to Figure 3 It can be seen that the excitation spectrum of the prepared tantalate near-infrared fluorescent material has two excitation peaks at 272nm and 428nm, which correspond to Ni 2+Broadband near-infrared characteristic excitation peak.

[0031] Example 2

[0032] A method for preparing a tantalate near-infrared fluorescent material, comprising the following preparation method:

[0033] (1) After mixing 24.95 mmol Ga2O3, 25 mmol Ta2O5, and 0.1 mmol NiO, the mixed powder is placed in an agate mortar, and then an appropriate amount of anhydrous ethanol is dropped into it and ground for 20 minutes; the volume ratio of the total mass of the mixed raw materials to the anhydrous ethanol is 1 g:6 ml.

[0034] (2) The ground powder is placed in a 70°C drying oven for half an hour, taken out and ground again until the material is in powder form, then the material is transferred to a corundum crucible, placed in a tubular furnace and heated at a rate of 5°C / min, sintered at 1300°C for 5 hours, and finally naturally cooled to room temperature to obtain a tantalate near-infrared fluorescent material.

[0035] The tantalate near-infrared fluorescent material prepared in Example 2 has a photoluminescence spectrum of broadband near-infrared light with an emission center at 1541 nm under 428 nm light excitation, and a relative luminescence intensity of 1.5 240 nm. Figure 4 .

[0036] Example 3

[0037] A method for preparing a tantalate near-infrared fluorescent material, comprising the following preparation method:

[0038] (1) After mixing 24.75 mmol Ga2O3, 25 mmol Ta2O5, and 0.5 mmol NiO, the mixed powder was placed in an agate mortar, and an appropriate amount of anhydrous ethanol was dropped into it and then ground for 60 minutes; the volume ratio of the total mass of the mixed raw materials to the anhydrous ethanol was 1 g:7 ml.

[0039] (2) The ground powder is placed in a 70°C drying oven for half an hour, taken out and ground again until the material is in powder form, then the material is transferred to a corundum crucible, placed in a tubular furnace and heated at a rate of 5°C / min, sintered at 1500°C for 1 hour, and finally naturally cooled to room temperature to obtain a tantalate near-infrared fluorescent material.

[0040] The tantalate near-infrared fluorescent material prepared in Example 3 has a photoluminescence spectrum of broadband near-infrared light with an emission center at 1566 nm under 428 nm light excitation, and a relative luminescence intensity of 1.5 240 nm. Figure 4 .

[0041] Comparative Example 1

[0042] A method for preparing a tantalate near-infrared fluorescent material, comprising the following preparation method:

[0043] (1) After mixing 25 mmol of Ga2O3 and 25 mmol of Ta2O5, the mixed powder was placed in an agate mortar, and then an appropriate amount of anhydrous ethanol was added and ground for 30 min;

[0044] (2) The ground powder is placed in a 70°C drying oven for half an hour, taken out and ground again until the material is in powder form, then the material is transferred to a corundum crucible, placed in a tubular furnace and heated at a rate of 5°C / min, sintered at 1500°C for 4 hours, and finally naturally cooled to room temperature to obtain a tantalate near-infrared fluorescent material.

[0045] The tantalate near-infrared fluorescent material prepared in Comparative Example 1 did not emit light under 428nm light excitation.

[0046] Comparative Example 2

[0047] A method for preparing a tantalate near-infrared fluorescent material, comprising the following preparation method:

[0048] (1) After mixing 24 mmol Ga2O3, 25 mmol Ta2O5, and 2 mmol NiO raw materials, the mixed powder was placed in an agate mortar, and then an appropriate amount of anhydrous ethanol was dropped into it and ground for 30 minutes;

[0049] (2) The ground powder is placed in a 70°C drying oven for half an hour, taken out and ground again until the material is in powder form, then the material is transferred to a corundum crucible, placed in a tubular furnace and heated at a rate of 5°C / min, sintered at 1500°C for 4 hours, and finally naturally cooled to room temperature to obtain a tantalate near-infrared fluorescent material.

[0050] The tantalate near-infrared fluorescent material prepared in Comparative Example 2 has a photoluminescence spectrum of broadband near-infrared light with an emission center at 1572nm under 428nm light excitation; compared with Examples 1-4, the luminescence intensity of the material in Comparative Example 2 is significantly reduced due to concentration quenching.

[0051] Comparative Example 3

[0052] A method for preparing a tantalate near-infrared fluorescent material, comprising the following preparation method:

[0053] (1) After mixing 24.9mmol Ga2O3, 25mmol Ta2O5 and 0.2mmol Cr2O3, the mixed powder was placed in an agate mortar, and an appropriate amount of anhydrous ethanol was dropped into it and then ground for 20 minutes; the volume ratio of the total mass of the raw material mixture to the anhydrous ethanol was 1g:6ml.

[0054] (2) The ground powder is placed in a 70°C drying oven for half an hour, taken out and ground again until the material is in powder form, then the material is transferred to a corundum crucible, placed in a tubular furnace and heated at a rate of 5°C / min, sintered at 1300°C for 5 hours, and finally naturally cooled to room temperature to obtain a tantalate near-infrared fluorescent material.

[0055] The tantalate near-infrared fluorescent material prepared in comparative example 3 has a photoluminescence spectrum of broadband near-infrared light with an emission center at 827nm under 428nm light excitation. The tantalate near-infrared fluorescent materials prepared in Examples 1-3 of the present invention have a wider half-width of the luminescence peak than the material in comparative example 3, including near-infrared region II and region III, and play an important role in the treatment of cancer, tumor cells, etc.

[0056] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A tantalate near-infrared fluorescent material, characterized in that: Its chemical formula is Ga 1-x TaO4:xNi 2+ , wherein 0<x≤0.01; the tantalate near-infrared fluorescent material generates near-infrared light with a luminescence center of 1541nm-1566nm under the excitation of light with a wavelength of 428nm, and the luminescence peak includes near-infrared second and third regions; The method for preparing the tantalate near-infrared fluorescent material comprises the following steps: (1) Mixing Ga2O3, Ta2O5 and NiO raw materials according to the stoichiometric ratio, adding anhydrous ethanol and grinding; (2) Then, the temperature is raised to 1300-1500° C. at a heating rate of 5° C. / min and calcined for 1-5 hours. After cooling, a tantalate near-infrared fluorescent material is obtained.

2. The tantalate near-infrared fluorescent material according to claim 1, characterized in that: The volume ratio of the total mass of the raw material mixture to anhydrous ethanol is 1g: (4-7)ml.

3. The tantalate near-infrared fluorescent material according to claim 1, characterized in that: The calcination atmosphere is at least one of air, nitrogen and argon.

4. The tantalate near-infrared fluorescent material according to claim 1, characterized in that: The purity of the Ga2O3, Ta2O5 and NiO raw materials is 99.99%.

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